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Acidic polymerized ionic liquid and preparation method and application thereof

A polymeric ionic liquid and acidic technology, which is applied in the field of multifunctional acidic polymeric ionic liquids, can solve the problems of limiting the use range of acidic ionic liquids, poor chemical stability, poor thermal stability, etc., and achieves the convenience of large-scale use and low price , the effect of improving efficiency

Active Publication Date: 2020-08-14
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, the use of inorganic carriers to support ionic liquids by means of adsorption has poor chemical stability during use, while traditional organic polymers as carriers have small specific surface area and poor thermal stability, which also limit the application range of acidic ionic liquids.
Although the current research on immobilized acidic ionic liquids is gradually deepening, how to prepare high-performance, green, high-stability acidic immobilized ionic liquids will still face severe challenges.

Method used

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  • Acidic polymerized ionic liquid and preparation method and application thereof
  • Acidic polymerized ionic liquid and preparation method and application thereof
  • Acidic polymerized ionic liquid and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under an inert atmosphere at 35°C, 0.4 g of tris(p-vinylphenyl)phosphine, 30 ml of tetrahydrofuran solvent, and 0.03 g of azobisisobutyronitrile were successively added into the single-necked flask as an initiator, and stirred at room temperature. The stirred solution is moved to a hydrothermal kettle, and the triphenylphosphine organic polymer is obtained by solvothermal polymerization. Add 0.134 g of 1,3-propane sultone and 20 ml of toluene to the above triphenylphosphine organic polymer, and stir at 35°C for 24 hours.

[0033] Add 3ml of p-toluenesulfonic acid to the above-mentioned reacted solution, stir and acidify at 35°C for 24h, and wash by centrifugation. After repeating the above acidification step three times, vacuum drying at 60°C for 5 h gave triphenylphosphine acidic solid ionic liquid, namely P PPh3-C-1 .

[0034] Toluene in Example 1 can be replaced by tetrahydrofuran, dichloromethane, methanol, ethanol, N,N dimethylformamide, N,N dimethylacetamide or ...

Embodiment 2

[0037] Under an inert atmosphere at 35°C, 0.4 g of tris(p-vinylphenyl)phosphine, 30 ml of tetrahydrofuran solvent, and 0.03 g of azobisisobutyronitrile were successively added into a single-necked flask as an initiator, and stirred at room temperature. The stirred solution is moved to a hydrothermal kettle, and the triphenylphosphine organic polymer is obtained by solvothermal polymerization. Add 0.134 g of 1,3-propane sultone and 20 ml of toluene to the above triphenylphosphine organic polymer, and stir and react at 35°C for 24 hours.

[0038] Add 2ml of trifluoromethanesulfonic acid to the above reacted solution, stir and acidify at 35°C for 24h, and wash by centrifugation. After repeating the above acidification step three times, vacuum drying at 60°C for 5 h gave triphenylphosphine acidic solid ionic liquid, P PPh3-F-1 .

[0039] The reaction formula is:

[0040]

[0041] Toluene in Example 2 can be replaced by tetrahydrofuran, methylene chloride, methanol, ethanol, ...

Embodiment 3

[0043]Under an inert atmosphere at 35°C, 0.4 g of tris(p-vinylphenyl)phosphorus, 0.134 g of 1,3-propane sultone, and 20 ml of toluene were successively added to the single-necked flask, and the reaction was stirred at 35°C for 24 hours, and then Add 0.03g of azobisisobutyronitrile to the solution as an initiator, stir for 0.5h, pour the liquid into a polytetrafluoroethylene-lined kettle, conduct solvent thermal polymerization at 100°C for 24h, and then vacuum dry at 60°C 10h.

[0044] Add 20ml of toluene to the above-reacted copolymer, stir for 0.5h, then add 2ml of p-toluenesulfonic acid, stir and acidify at 35°C for 24h, and wash by centrifugation. After repeating the above acidification step three times, vacuum drying at 60°C for 5 h yielded triphenylphosphine acidic solid ionic liquid, P PPh3-C-2 .

[0045] Its reaction formula is:

[0046]

[0047] Toluene in embodiment 3 can be replaced by tetrahydrofuran, dichloromethane, methyl alcohol, ethanol, N,N dimethylforma...

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Abstract

The invention discloses an acidic polymerized ionic liquid and preparation methods thereof. The preparation method 1 comprises the steps that firstly, a phosphine ligand containing vinyl is subjectedto solvothermal self-polymerization or copolymerized with other monomers containing vinyl to prepare a porous organic polymer, then 1, 3-propane sultone is added for a reaction, and finally acidification is performed to obtain the acidic polymerized ionic liquid. The preparation method 2 comprises the following steps: reacting a phosphine ligand containing vinyl with 1, 3-propane sultone, then self-polymerizing or copolymerizing with other monomers containing vinyl, and finally acidifying. The preparation methods provided by the invention are simple in process, less in three wastes and low incost, and the obtained acidic solid-state polymerized ionic liquid has a high specific surface area, a hierarchical pore structure and excellent thermal stability and chemical stability, and can be used as an electrode material, a gas separation material, a catalyst, a catalyst carrier and the like.

Description

technical field [0001] The invention belongs to the field of polymer functional materials, and relates to a multifunctional acidic polymeric ionic liquid, a preparation method and application thereof. Background technique [0002] Porous materials have experienced the development process from natural acquisition to artificial synthesis, from inorganic to organic materials, and play an important role in the fields of catalysis, gas separation and optoelectronics. In recent decades, porous organic materials, such as porous organic polymers (POPs), metal-organic frameworks (MOFs), and covalent organic frameworks (COFs), have been widely used in many fields and have attracted great attention from researchers at home and abroad. . Among them, POPs have become a research hotspot due to their large specific surface area, hierarchical pore structure, adjustable pore size, functional group modification, and good physical and chemical stability. [0003] Ionic liquids refer to organ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F130/02C08F230/02C08F8/36
CPCC08F8/36C08F130/02C08F230/02
Inventor 陈兴坤丁云杰王赛赛
Owner ZHEJIANG NORMAL UNIVERSITY